CN105803395A - Preparation method for multi-layer Ni/BaTiO3 thin film capable of reducing dielectric losses - Google Patents
Preparation method for multi-layer Ni/BaTiO3 thin film capable of reducing dielectric losses Download PDFInfo
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- CN105803395A CN105803395A CN201610194051.1A CN201610194051A CN105803395A CN 105803395 A CN105803395 A CN 105803395A CN 201610194051 A CN201610194051 A CN 201610194051A CN 105803395 A CN105803395 A CN 105803395A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/08—Oxides
- C23C14/088—Oxides of the type ABO3 with A representing alkali, alkaline earth metal or Pb and B representing a refractory or rare earth metal
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention relates to a preparation method for a multi-layer Ni/BaTiO3 thin film capable of decreasing dielectric losses and belongs to the technical field of dielectric substance synthesizing. The preparation method comprises the steps that firstly, nano BaTiO3 powder is pressed into a target material; secondly, the target material and a Ni substrate are fixed to magnetron sputtering equipment to complete sputtering; and finally, the target material and the Ni substrate are subjected to heat treatment through a tube furnace, and the finished multi-layer Ni/BaTiO3 thin film is prepared. The Ni/BaTiO3 thin film prepared through the preparation method is of a multi-layer thin film structure, not only can migration of oxygen vacancies be hindered, but also the internal pressure stress of the surface of the BaTiO3 thin film can be increased; therefore, the functions of decreasing the dielectric losses and increasing dielectric constants can be achieved, and the problems of current leakage, dielectric loss increasing and even thin film failure caused by oxygen vacancies produced in the preparation process of an existing BaTiO3 thin film are solved; and positive application prospects of the high-dielectric-constant BaTiO3 thin film in the fields of inserted capacitors, high-energy-storage elements and the like are achieved.
Description
Technical field
The present invention relates to a kind of multilamellar Ni/BaTiO that can reduce dielectric loss3The preparation method of thin film；Belong to electrolyte material
Material synthesis technical field.
Background technology
The BaTiO of high-k3Thin film has important application prospect in the field such as embedded capacitance and high energy-storage travelling wave tube,
Particularly Direct precipitation BaTiO on the base metal substrate such as Ni, Cu3Thin film, attracts wide attention in recent years, especially, because of lining
Residual stress that between the end and thin film, mismatch causes and the leakage current that Lacking oxygen migration, redistribution etc. cause have attracted people especially
Sight.
BaTiO3Thin film can produce Lacking oxygen, the Lacking oxygen for block materials, in thin film in preparation process
Concentration is relatively big, causes leakage current and dielectric loss to increase, even can cause the failure behaviour of thin film.Lacking oxygen moving in the film
Shifting can be hindered by crystal boundary, electrode-film interface, and research shows that Lacking oxygen crosses the back-to-back pair of Schottky that crystal boundary is formed
Energy needed for potential barrier is less than the potential barrier crossed needed for membrane electrode interface.Multilamellar BaTiO is found in experimentation3Thin
The barrier height at the homogeneity interface that film is formed also is greater than the back-to-back pair of schottky barrier height that crystal boundary is formed.Additionally, grind
Study carefully and show that face internal pressure stress can improve BaTiO3The dielectric constant (being parallel to substrate surface) of base-multilayer ceramic capacitor.And
Along with the increase of film thickness, residual compressive stress is on a declining curve.It is therefore desirable to research and develop a kind of to hinder the migration of Lacking oxygen,
Increase BaTiO3Pellicular front internal pressure stress, can play simultaneously and reduce dielectric loss and improve the plural layers of dielectric constant effect
Structure.
Summary of the invention
It is an object of the invention to: provide one to prepare simply, it is possible to reduce thin-film dielectric loss and improve thin-film dielectric
Multilamellar Ni/BaTiO that can reduce dielectric loss of constant3The preparation method of thin film.
The technical scheme is that
A kind of Ni/BaTiO that can reduce dielectric loss3The preparation method of plural layers, it is characterised in that: it includes following step
Suddenly；
1), by nanometer BaTiO3Powder (30nm, 99.9%, 1kg) is 1000oThe BaTiO of a diameter of 75mm it is pressed under C3Target；
2), by BaTiO3Target is respectively washed 5min with in dehydrated alcohol, deionized water successively, with by BaTiO3Target material surface
Impurity cleaning is clean, the most in an oven by BaTiO3Target is dried；Standby；
3), by Ni substrate (10 × 10 × 1mm3 ) at N2Atmosphere, 800-1000oHeat treatment 30min under the conditions of C, so that Ni
The crystal grain of substrate is grown up, and is then polished Ni substrate, till becoming minute surface；
4), by Ni substrate ultrasonic 5min in dehydrated alcohol, the most ultrasonic 5min after polishing, finally take
Go out substrate and use N2Air-blowing is done；To ensure the cleannes of Ni substrate；
5), the Ni substrate dried up is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, simultaneously at magnetron sputtering apparatus
Middle inner cavity chamber fixes BaTiO3Target, then magnetron sputtering apparatus inner chamber is evacuated to vacuum is 10-4Pa；
6), in equipment, it is passed through Ar and O2(with Ar as reference, O2It is biased in 10−7With 10−8 Between atm) until operating pressure reaches
To 2.2Pa, and set the sputtering power of sputtering equipment as 144W, underlayer temperature as 350-450oC, Ni substrate rotary speed is
The sputtering parameter of 10-20rpm carries out sputtering for the first time；
7), in first time sputter procedure, the sputtering thickness of thin film is detected at any time, until it reaches set thickness, after having sputtered,
Take out sample after cooling to room temperature and be placed in sample box that (sample box to process, it is to avoid the dust adsorption of the inside is to thin film
Surface, affects the test result of thin film), to prevent film surface from cut occurring；
8), first time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until the air quilt of the inside
Drive out of clean, then tube furnace is warmed up to 750oC, programming rate is 10 oC/min, 750oC heated at constant temperature 30min is carried out
Heat treatment, then drops to room temperature, and cooling rate is 10 oC/min；
9), heat treatment will be completed after sputtered samples carry out second time sputter, the Ni underlayer temperature in sputtering parameter sets for the second time
It is set to 380-480oC, the sputtering power of sputtering equipment be 144W, Ni substrate rotary speed be 10-20rpm,
10), second time sputtered after sputtered samples is placed in tube furnace, be passed through protective gas N22min, until in
The air in face is forced out totally, then tube furnace being warmed up to 750oC, programming rate is 10 oC/min, 750oC heated at constant temperature
30min, then drops to room temperature, and cooling rate is 10 oC/min, Ni/BaTiO3Plural layers finished product.
Thin film can sputter four layers as required, in every layer of sputter procedure based on primary Ni substrate sputter temperature,
Improve Ni substrate sputter temperature 30 every timeoC。
It is an advantage of the current invention that:
Use the Ni/BaTiO of the inventive method preparation synthesis3Thin film has multi-layer film structure；This multi-layer film structure is not only
The migration of Lacking oxygen can be hindered, it is also possible to increase BaTiO3Pellicular front internal pressure stress, therefore can play reduction dielectric loss
With the effect of raising dielectric constant, solve existing BaTiO3Thin film produces Lacking oxygen because of preparation, military service and causes leakage current, Jie
Electrical loss increases, the problem even lost efficacy；BaTiO to high-k3Thin film is at embedded capacitance and high energy-storage travelling wave tube etc.
There is positive application prospect in field.
For showing that the present invention prepares the Ni/BaTiO of synthesis3The parameters performance indications of thin film, the Ni/ to preparation synthesis
BaTiO3Thin film has carried out detection test, and concrete outcome is as follows:
Accompanying drawing explanation
Fig. 1 is the relation corresponding diagram in preparation process of the present invention between sputtering time and film thickness；
Fig. 2 is the Ni/BaTiO of the different numbers of plies prepared by the present invention3The capacitance density of thin film and dielectric loss relation corresponding diagram.
Detailed description of the invention
Embodiment 1:
By nanometer BaTiO3Powder (30nm, 99.9%, 1kg) is 1000oThe BaTiO of a diameter of 75mm it is pressed under C3Target；Will
BaTiO3Target is respectively washed 5min with in dehydrated alcohol, deionized water successively, with by BaTiO3The impurity cleaning of target material surface is dry
Only, the most in an oven by BaTiO3Target is dried；Standby；By Ni substrate (10 × 10 × 1mm3 ) at N2Atmosphere,
800oHeat treatment 30min under the conditions of C, so that the crystal grain of Ni substrate is grown up, is then polished Ni substrate, until becoming minute surface
Till.By Ni substrate ultrasonic 5min in dehydrated alcohol, the most ultrasonic 5min after polishing, finally take out
Substrate also uses N2Air-blowing is done；To ensure the cleannes of Ni substrate.In the Ni substrate dried up is fixed in magnetron sputtering apparatus
On the sample stage of chamber, inner cavity chamber fixes in magnetron sputtering apparatus BaTiO simultaneously3Target, then by magnetron sputtering apparatus
It is 10 that inner chamber is evacuated to vacuum-4Pa.It is passed through Ar and O in magnetron sputtering apparatus2(with Ar as reference, O2It is biased in 10−7With 10−8 Between atm) until operating pressure reaches 2.2Pa, and set the sputtering power of sputtering equipment as 144W, underlayer temperature as
350oC, Ni substrate rotary speed is that the sputtering parameter of 10-20rpm carries out sputtering for the first time.In first time sputter procedure, with
Time detection thin film sputtering thickness, until it reaches set thickness, after sputter, taking-up sample being placed on after cooling to room temperature
In sample box (sample box to process, it is to avoid the dust adsorption of the inside to film surface, affects the test result of thin film), in case
Only there is cut in film surface.First time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until
The air of the inside is forced out totally, then tube furnace being warmed up to 750oC, programming rate is 10 oC/min, 750oC constant temperature adds
Hot 30min carries out heat treatment, then drops to room temperature, and cooling rate is 10 oC/min；Sputtered samples after completing heat treatment is entered
Row second time sputtering, the Ni underlayer temperature in sputtering parameter is set to 380 for the second timeoC, the sputtering power of sputtering equipment is
144W, Ni substrate rotary speed is 10-20rpm, and sputtered samples is placed in tube furnace after having sputtered by second time, is passed through guarantor
Protecting property gas N22min, until the air of the inside is forced out totally, then tube furnace being warmed up to 750oC, programming rate is 10oC/min, 750oC heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 oC/min, Ni/BaTiO3Multilamellar
Finished film.
Embodiment 2:
By nanometer BaTiO3Powder (30nm, 99.9%, 1kg) is 1000oThe BaTiO of a diameter of 75mm it is pressed under C3Target；Will
BaTiO3Target is respectively washed 5min with in dehydrated alcohol, deionized water successively, with by BaTiO3The impurity cleaning of target material surface is dry
Only, the most in an oven by BaTiO3Target is dried；Standby；By Ni substrate (10 × 10 × 1mm3 ) at N2Atmosphere,
900oHeat treatment 30min under the conditions of C, so that the crystal grain of Ni substrate is grown up, is then polished Ni substrate, until becoming minute surface
Till.By Ni substrate ultrasonic 5min in dehydrated alcohol, the most ultrasonic 5min after polishing, finally take out
Substrate also uses N2Air-blowing is done；To ensure the cleannes of Ni substrate.In the Ni substrate dried up is fixed in magnetron sputtering apparatus
On the sample stage of chamber, inner cavity chamber fixes in magnetron sputtering apparatus BaTiO simultaneously3Target, then by magnetron sputtering apparatus
It is 10 that inner chamber is evacuated to vacuum-4Pa.It is passed through Ar and O in magnetron sputtering apparatus2(with Ar as reference, O2It is biased in 10−7With 10−8 Between atm) until operating pressure reaches 2.2Pa, and set the sputtering power of sputtering equipment as 144W, underlayer temperature as
400oC, Ni substrate rotary speed is that the sputtering parameter of 10-20rpm carries out sputtering for the first time.In first time sputter procedure, with
Time detection thin film sputtering thickness, until it reaches set thickness, after sputter, taking-up sample being placed on after cooling to room temperature
In sample box (sample box to process, it is to avoid the dust adsorption of the inside to film surface, affects the test result of thin film), in case
Only there is cut in film surface.First time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until
The air of the inside is forced out totally, then tube furnace being warmed up to 750oC, programming rate is 10 oC/min, 750oC constant temperature adds
Hot 30min carries out heat treatment, then drops to room temperature, and cooling rate is 10 oC/min；Sputtered samples after completing heat treatment is entered
Row second time sputtering, the Ni underlayer temperature in sputtering parameter is set to 430 for the second timeoC, the sputtering power of sputtering equipment is
144W, Ni substrate rotary speed is 10-20rpm, and sputtered samples is placed in tube furnace after having sputtered by second time, is passed through guarantor
Protecting property gas N22min, until the air of the inside is forced out totally, then tube furnace being warmed up to 750oC, programming rate is 10oC/min, 750oC heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 oC/min, Ni/BaTiO3Multilamellar
Finished film.
Embodiment 3:
By nanometer BaTiO3Powder (30nm, 99.9%, 1kg) is 1000oThe BaTiO of a diameter of 75mm it is pressed under C3Target；Will
BaTiO3Target is respectively washed 5min with in dehydrated alcohol, deionized water successively, with by BaTiO3The impurity cleaning of target material surface is dry
Only, the most in an oven by BaTiO3Target is dried；Standby；By Ni substrate (10 × 10 × 1mm3 ) at N2Atmosphere,
1000oHeat treatment 30min under the conditions of C, so that the crystal grain of Ni substrate is grown up, is then polished Ni substrate, until Cheng Jing
Till face.By Ni substrate ultrasonic 5min in dehydrated alcohol, the most ultrasonic 5min after polishing, finally take
Go out substrate and use N2Air-blowing is done；To ensure the cleannes of Ni substrate.The Ni substrate dried up is fixed in magnetron sputtering apparatus
On the sample stage of inner cavity chamber, inner cavity chamber fixes in magnetron sputtering apparatus BaTiO simultaneously3Target, then magnetron sputtering is set
It is 10 that standby inner chamber is evacuated to vacuum-4Pa.It is passed through Ar and O in magnetron sputtering apparatus2(with Ar as reference, O2It is biased in 10−7With
10−8 Between atm) until operating pressure reaches 2.2Pa, and set the sputtering power of sputtering equipment as 144W, underlayer temperature as
450oC, Ni substrate rotary speed is that the sputtering parameter of 10-20rpm carries out sputtering for the first time.In first time sputter procedure, with
Time detection thin film sputtering thickness, until it reaches set thickness, after sputter, taking-up sample being placed on after cooling to room temperature
In sample box (sample box to process, it is to avoid the dust adsorption of the inside to film surface, affects the test result of thin film), in case
Only there is cut in film surface.First time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until
The air of the inside is forced out totally, then tube furnace being warmed up to 750oC, programming rate is 10 oC/min, 750oC constant temperature adds
Hot 30min carries out heat treatment, then drops to room temperature, and cooling rate is 10 oC/min；Sputtered samples after completing heat treatment is entered
Row second time sputtering, the Ni underlayer temperature in sputtering parameter is set to 480 for the second timeoC, the sputtering power of sputtering equipment is
144W, Ni substrate rotary speed is 10-20rpm, and sputtered samples is placed in tube furnace after having sputtered by second time, is passed through guarantor
Protecting property gas N22min, until the air of the inside is forced out totally, then tube furnace being warmed up to 750oC, programming rate is 10oC/min, 750oC heated at constant temperature 30min, then drops to room temperature, and cooling rate is 10 oC/min, Ni/BaTiO3Multilamellar
Finished film.
Claims (1)
1. the Ni/BaTiO that can reduce dielectric loss3The preparation method of plural layers, it is characterised in that: it includes following step
Suddenly；
1), by nanometer BaTiO3Powder is 1000oThe BaTiO of a diameter of 75mm it is pressed under C3Target；
2), by BaTiO3Target is respectively washed 5min with in dehydrated alcohol, deionized water successively, with by BaTiO3Target material surface
Impurity cleaning is clean, the most in an oven by BaTiO3Target is dried；Standby；
3), by Ni substrate at N2Atmosphere, 800-1000oHeat treatment 30min under the conditions of C, so that the crystal grain of Ni substrate is grown up, so
Afterwards Ni substrate is polished, till becoming minute surface；
4), by Ni substrate ultrasonic 5min in dehydrated alcohol, the most ultrasonic 5min after polishing, finally take
Go out substrate and use N2Air-blowing is done；To ensure the cleannes of Ni substrate；
5), the Ni substrate dried up is fixed in magnetron sputtering apparatus on the sample stage of inner cavity chamber, simultaneously at magnetron sputtering apparatus
Middle inner cavity chamber fixes BaTiO3Target, then magnetron sputtering apparatus inner chamber is evacuated to vacuum is 10-4Pa；
6), in equipment, it is passed through Ar and O2Until operating pressure reaches 2.2Pa, and set the sputtering power of sputtering equipment as 144W,
Underlayer temperature is 350-450oC, Ni substrate rotary speed is that the sputtering parameter of 10-20rpm carries out sputtering for the first time；
7), in first time sputter procedure, the sputtering thickness of thin film is detected at any time, until it reaches set thickness, after having sputtered,
Take out sample after cooling to room temperature and be placed in sample box, to prevent film surface from cut occurring；
8), first time sputtered samples is placed in tube furnace, is passed through protective gas N2About 2min, until the air quilt of the inside
Drive out of clean, then tube furnace is warmed up to 750oC, programming rate is 10 oC/min, 750oC heated at constant temperature 30min is carried out
Heat treatment, then drops to room temperature, and cooling rate is 10 oC/min；
9), heat treatment will be completed after sputtered samples carry out second time sputter, the Ni underlayer temperature in sputtering parameter sets for the second time
It is set to 380-480oC, the sputtering power of sputtering equipment be 144W, Ni substrate rotary speed be 10-20rpm,
10), second time sputtered after sputtered samples is placed in tube furnace, be passed through protective gas N22min, until in
The air in face is forced out totally, then tube furnace being warmed up to 750oC, programming rate is 10 oC/min, 750oC heated at constant temperature
30min, then drops to room temperature, and cooling rate is 10 oC/min, Ni/BaTiO3Plural layers finished product.
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| CN201610194051.1A CN105803395B (en) | 2016-03-31 | 2016-03-31 | A kind of preparation method for the multilayer Ni/BaTiO3 films that can reduce dielectric loss |
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| CN201610194051.1A CN105803395B (en) | 2016-03-31 | 2016-03-31 | A kind of preparation method for the multilayer Ni/BaTiO3 films that can reduce dielectric loss |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106191776A (en) * | 2016-08-20 | 2016-12-07 | 苏州思创源博电子科技有限公司 | A kind of preparation method of molybdenum alloy barium titanate film |
| CN106222620A (en) * | 2016-08-20 | 2016-12-14 | 苏州思创源博电子科技有限公司 | A kind of preparation method of the tungsten nickel dielectric substance possessing barium titanate film |
| CN106319464A (en) * | 2016-08-20 | 2017-01-11 | 苏州思创源博电子科技有限公司 | Method for preparing barium titanate film on tungsten alloy substrate |
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| CN106319464A (en) * | 2016-08-20 | 2017-01-11 | 苏州思创源博电子科技有限公司 | Method for preparing barium titanate film on tungsten alloy substrate |
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| CN105803395B (en) | 2018-05-25 |
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